CN101993438B - Method for extracting mangiferin and total saponins of rhizoma anemarrhenae from rhizoma anemarrhenae - Google Patents
Method for extracting mangiferin and total saponins of rhizoma anemarrhenae from rhizoma anemarrhenae Download PDFInfo
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- CN101993438B CN101993438B CN200910194674.9A CN200910194674A CN101993438B CN 101993438 B CN101993438 B CN 101993438B CN 200910194674 A CN200910194674 A CN 200910194674A CN 101993438 B CN101993438 B CN 101993438B
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- wind
- weed
- rhizoma anemarrhenae
- mangiferin
- total saponins
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- AEDDIBAIWPIIBD-ZJKJAXBQSA-N mangiferin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1C1=C(O)C=C(OC=2C(=CC(O)=C(O)C=2)C2=O)C2=C1O AEDDIBAIWPIIBD-ZJKJAXBQSA-N 0.000 title claims abstract description 68
- YWQSXCGKJDUYTL-UHFFFAOYSA-N Mangiferin Natural products CC(CCC=C(C)C)C1CC(C)C2C3CCC4C(C)(C)CCCC45CC35CCC12C YWQSXCGKJDUYTL-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229940043357 mangiferin Drugs 0.000 title claims abstract description 34
- 229930182490 saponin Natural products 0.000 title claims abstract description 29
- 150000007949 saponins Chemical class 0.000 title claims abstract description 29
- 235000017709 saponins Nutrition 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000000605 extraction Methods 0.000 claims abstract description 22
- 238000001556 precipitation Methods 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000003814 drug Substances 0.000 claims abstract description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 45
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 23
- 239000007788 liquid Substances 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 22
- 239000000706 filtrate Substances 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 10
- 238000002425 crystallisation Methods 0.000 claims description 8
- 230000008025 crystallization Effects 0.000 claims description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 239000000284 extract Substances 0.000 claims description 6
- 239000012452 mother liquor Substances 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 235000012054 meals Nutrition 0.000 claims description 4
- 239000001397 quillaja saponaria molina bark Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 239000006228 supernatant Substances 0.000 claims description 2
- 239000012141 concentrate Substances 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 4
- 238000001953 recrystallisation Methods 0.000 abstract description 4
- 238000000926 separation method Methods 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 2
- 238000009833 condensation Methods 0.000 abstract 1
- 230000005494 condensation Effects 0.000 abstract 1
- 238000004821 distillation Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 5
- 238000005267 amalgamation Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 241000605447 Anemarrhena Species 0.000 description 1
- 241000208340 Araliaceae Species 0.000 description 1
- 241000380450 Danaus melanippus Species 0.000 description 1
- 241000721047 Danaus plexippus Species 0.000 description 1
- 206010013954 Dysphoria Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 206010018473 Glycosuria Diseases 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229930191283 anemarrhena Natural products 0.000 description 1
- 230000000702 anti-platelet effect Effects 0.000 description 1
- 230000001754 anti-pyretic effect Effects 0.000 description 1
- 239000003146 anticoagulant agent Substances 0.000 description 1
- 239000002221 antipyretic Substances 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 210000001124 body fluid Anatomy 0.000 description 1
- 239000010839 body fluid Substances 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000002279 cholagogic effect Effects 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 230000002218 hypoglycaemic effect Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 239000013558 reference substance Substances 0.000 description 1
- 230000000452 restraining effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 230000035807 sensation Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 208000010110 spontaneous platelet aggregation Diseases 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 230000035922 thirst Effects 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
- 235000021228 wine soup Nutrition 0.000 description 1
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- Steroid Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention belongs to the field of medicine preparation, and in particular relates to a method for extracting mangiferin and total saponins of rhizoma anemarrhenae from rhizoma anemarrhenae, which mainly comprises the following steps of: water or diluted alcohol extraction, condensation, alcohol precipitation, filtering, dry by distillation and re-crystallization. The separation process related to the invention has the advantages of simplicity and convenience, economical efficiency and reliability.
Description
Technical field
The invention belongs to medicine preparation field, relate to the extraction preparation method of medicinal material effective constituent, be specifically related to a kind of method of extracting Mangiferin and Rhizoma Anemarrhenae total saponins from the wind-weed.
Background technology
The wind-weed is the dry rhizome of the liliaceous plant wind-weed (Anemarrhena asphodeloiides Bge).Bitter, sweet, cold in nature, enter lung, stomach, kidney channel, there is heat-clearing and fire-purging, promote the production of body fluid and the effect such as moisturize, cure mainly dysphoria with smothery sensation, quench one's thirst.Pharmacological research shows that the wind-weed has the effects such as antipyretic, hypoglycemic, cholagogic, anti-platelet aggregation.Its saponin constituent, Mangiferin have blood sugar reducing function, in the treatment diabetes decoctions such as thirsty clear, the woods board glycosuria capsule of the good wine soup of use, white tiger ginseng decoction, sugar, glucemia be peaceful clinically or prescription, wind-weed Chang Zuowei monarch drug in a prescription is used, by related data, analyze, the p-glucosidase activity half of Rhizoma Anemarrhenae total saponins restraining effect dosage is about 10 times of Mangiferin, and Mangiferin accounts for 10% in Rhizoma Anemarrhenae total saponins.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method of extracting Mangiferin and Rhizoma Anemarrhenae total saponins from the wind-weed, adopt the method can effectively from the wind-weed, isolate Rhizoma Anemarrhenae total saponins and Mangiferin, and under this prerequisite, make sepn process easy, economical, reliable.For this object of the invention can be realized smoothly, the present invention has adopted following technical scheme:
From the wind-weed, extract a method for Mangiferin and Rhizoma Anemarrhenae total saponins, its step comprises:
A, water or ethanol-extracted rhizoma ane marrhenae medicine materical crude slice or meal, concentrated gained extracting solution, carries out alcohol precipitation to the extracting solution after concentrated, obtains filtrate part and precipitation part;
B, filtrate is partly concentrated, then use n-butanol extraction, obtain the first extraction liquid;
C, precipitation part add alkali lye alkalization, stir one hour, and centrifugal, supernatant liquor neutralizes with diluted acid, after concentrating under reduced pressure, with n-butanol extraction, obtains the second extraction liquid;
D, merge the first extraction liquid and the second extraction liquid, be concentrated into dryly, obtain the thick total saponin powder of the wind-weed;
E, with the thick total saponin powder of a small amount of lower alcohol heating for dissolving wind-weed, place, crystallization, obtain mangiferin crystal and mother liquor;
F, condensing crystal mother liquor are to the dry Rhizoma Anemarrhenae total saponins that obtains.
Rhizoma ane marrhenae described in the technical program can be wind-weed medicine materical crude slice, or wind-weed meal.
Because Rhizoma Anemarrhenae total saponins is soluble in lower alcohol, and the solubleness of Mangiferin in lower alcohol is lower, particularly when temperature is lower, based on this point, alcohol precipitation of the present invention is to add lower alcohol in this concentrated rear extracting solution, makes content shared mass percent in adding the purification liquid of lower alcohol of lower alcohol reach 60%～75%.Lower alcohol is preferably methyl alcohol or ethanol.
Because Mangiferin is containing acidic phenol hydroxyl, utilize alkali lye to process precipitation part, can be by a small amount of residual Mangiferin in this part the water-soluble liquid of form with salify, reach the effect that makes full use of effective ingredient, for extracting comprehensively, further improve the output of Rhizoma Anemarrhenae total saponins and Mangiferin, the present invention is that mass percent concentration is a kind of in 1%～5% sodium hydroxide, potassium hydroxide, sodium carbonate or sodium bicarbonate to the alkali lye in the treatment step of precipitation part.
Lower alcohol or water that the present invention is is 40%～70% with mass percent concentration extract rhizoma ane marrhenae as extraction agent, the proportion 1.1～1.3 of the concentrated rear extracting solution in described a step,
The polarity of considering Rhizoma Anemarrhenae total saponins and Mangiferin is high, and according to the similar principle that mixes, the present invention selects propyl carbinol to extract.
The inventive method also comprises the recrystallization to mangiferin crystal described in e step, further to improve the purity of Mangiferin.
To sum up, solubleness inconsistent feature that the present invention has utilized Rhizoma Anemarrhenae total saponins and Mangiferin to show in some solvent, both have been carried out to effective separation, although this separation method all operations is the general operation in this area, but obtained good separating effect, and obtained highly purified Mangiferin, thereby it is low to make the inventive method possess cost, easy, be easy to the feature that extension is produced, in addition, the present invention has also added precipitation partially disposed step in technical process, has improved the yield of product.
Embodiment
Embodiment 1
Below the present invention will be further described:
Get 1kg wind-weed medicine materical crude slice, by 10 liter water refluxing extraction, extract altogether 3 times, each 1.5 hours, merge 3 times water extraction liquid, filter, it is 1.1～1.3 that filtrate decompression is concentrated into proportion, add alcohol adjusting and make its spirituosity 65%～70%, place 24 hours, precipitation, filters, obtain filtrate part and precipitation part, filtrate part concentrating under reduced pressure obtains concentrated solution;
Precipitation part, is placed in 60 ℃～70 ℃ stirring in water bath 1 hour with 2% sodium hydroxide, filters, and alkaline filtrate is adjusted after pH to 7 with dilute hydrochloric acid, and concentrating under reduced pressure and the merging of aforementioned concentrated solution, obtain amalgamation liquid;
Propyl carbinol 300ml is used in amalgamation liquid n-butanol extraction 3 times at every turn, merges butanol extraction liquid, with a small amount of water backwash once;
Gained n-butanol layer is evaporated to dry, obtains the thick total saponins powder of the wind-weed;
With the thick total saponins powder of the 100ml methyl alcohol heating for dissolving wind-weed, then place 24 hours, crystallization, filters, crystallization is washed once with a small amount of methyl alcohol, crystallization with a small amount of methyl alcohol again recrystallization once, obtain faint yellow Mangiferin sterling 7.1g, yield 0.71%;
Methanol mother liquor evaporate to dryness, obtains off-white color powder 32.5g Rhizoma Anemarrhenae total saponins, yield 3.25%.
Embodiment 2
Get 1kg wind-weed meal, with 10 liter 70% alcohol reflux, extract altogether 3 times, each 1.5 hours, merge 3 times Diluted Alcohol extracting solution, filter, it is 1.1～1.3 that filtrate decompression is concentrated into proportion, add alcohol adjusting and make spirituosity 65%～70%, place 24 hours, precipitation, filters, obtain filtrate part and precipitation part, filtrate part concentrating under reduced pressure obtains concentrated solution;
Precipitation, is placed in 60 ℃～70 ℃ stirring in water bath 1 hour with 2% sodium hydroxide, filters, and alkaline filtrate is adjusted after pH to 7 with dilute hydrochloric acid, and concentrating under reduced pressure and the merging of aforementioned concentrated solution, obtain amalgamation liquid;
Propyl carbinol 300ml is used in amalgamation liquid n-butanol extraction 3 times at every turn, merges butanol extraction liquid, with a small amount of water backwash once;
Gained n-butanol layer reclaim under reduced pressure, to dry, obtains the thick total saponins powder of the wind-weed;
By 100ml methyl alcohol heating for dissolving, place 24 hours, crystallization, filters, crystallization is washed once with a small amount of methyl alcohol, crystallization with a small amount of methyl alcohol again recrystallization once, obtain faint yellow Mangiferin sterling 7.8g, yield 0.78%;
Methanol mother liquor evaporate to dryness, obtains off-white color powder 37g Rhizoma Anemarrhenae total saponins, yield 3.7%.
For ease of Mangiferin in comparing embodiment 1 and embodiment 2 at the extraction yield of the whole wind-weed, need to measure the contained ratio of Mangiferin in the whole wind-weed, the mensuration of Mangiferin content can be adopted with the following method and be carried out: (magazine is analyzed in the analysis of the method reference drug, 2007,27 (9): the method for describing on 1478)
1. test condition
High performance liquid chromatograph: Agilent 1100, Elite-ODS chromatographic column (4.0mm * 150mm, 5 μ m)
Moving phase: MeOH-0.1% phosphoric acid liquid (27: 73v/v)
Flow velocity: 1.0ml/min
Detect wavelength: 316nm
Column temperature: room temperature
Sampling volume: 10 μ l
2. wind-weed sample liquid preparation
Get dry medicinal material powder (80 order) 1g of the wind-weed, accurately weighed 1.0508g, adds methyl alcohol appropriate, reflux 1 hour, cooling, filter, filter residue methanol wash 3 times, methyl alcohol filtrate is quantitatively to 100ml measuring bottle, shake up, through 0.45 μ m millipore filtration, as trial-product liquid.
Mangiferin sample weighs after 6 hours through 70 ℃ of drying under reduced pressure, and Mangiferin reference substance is made into the solution of 42.8 μ g/ml.
In rhizoma ane marrhenae, Mangiferin content is 1.28% after measured, and gained sample Mangiferin purity is respectively 96% and 97%, and it extracts yield from medicinal material is 55.5% and 66.4%.
Should be appreciated that those skilled in the art can make various changes or modifications the utility model after having read above-mentioned teachings of the present utility model, these equivalent form of values fall within the application's appended claims limited range equally.
Claims (4)
1. from the wind-weed, extract a method for Mangiferin and Rhizoma Anemarrhenae total saponins, it is characterized in that the method step comprises:
A, water or mass percent concentration are 40%～70% lower alcohol extraction wind-weed medicine materical crude slice or wind-weed meal, and described lower alcohol is methyl alcohol or ethanol; Concentrated gained extracting solution, carries out alcohol precipitation to the extracting solution after concentrated, filters, and obtains filtrate part and precipitation part;
B, filtrate is partly concentrated, then use n-butanol extraction, obtain the first extraction liquid;
C, precipitation part add alkali lye alkalization, stir one hour, and centrifugal, supernatant liquor neutralizes with diluted acid, after concentrating under reduced pressure, with n-butanol extraction, obtain the second extraction liquid;
D, merging the first extraction liquid and the second extraction liquid are concentrated into dry, obtain the thick total saponin powder of the wind-weed;
E, with the thick total saponins powder of a small amount of lower alcohol heating for dissolving wind-weed, place, crystallization, obtain mangiferin crystal and mother liquor; Described lower alcohol is methyl alcohol or ethanol;
F, condensing crystal mother liquor are to the dry Rhizoma Anemarrhenae total saponins that obtains.
2. a kind of method of extracting Mangiferin and Rhizoma Anemarrhenae total saponins from the wind-weed according to claim 1, is characterized in that the proportion 1.1～1.3 that concentrates rear extracting solution in a step.
3. a kind of method of extracting Mangiferin and Rhizoma Anemarrhenae total saponins from the wind-weed according to claim 1, it is characterized in that described alcohol precipitation is to add lower alcohol in this concentrated rear extracting solution, make content shared mass percent in adding the purification liquid of lower alcohol of lower alcohol reach 60%～75%, described lower alcohol is methyl alcohol or ethanol.
4. a kind of method of extracting Mangiferin and Rhizoma Anemarrhenae total saponins from the wind-weed according to claim 1, is characterized in that to the alkali lye in the treatment step of precipitation part being that mass percent is a kind of in 1%～5% sodium hydroxide, potassium hydroxide, sodium carbonate or sodium bicarbonate.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910194674.9A CN101993438B (en) | 2009-08-27 | 2009-08-27 | Method for extracting mangiferin and total saponins of rhizoma anemarrhenae from rhizoma anemarrhenae |
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| CN200910194674.9A CN101993438B (en) | 2009-08-27 | 2009-08-27 | Method for extracting mangiferin and total saponins of rhizoma anemarrhenae from rhizoma anemarrhenae |
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| CN101993438B true CN101993438B (en) | 2014-04-09 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103349724A (en) * | 2013-08-02 | 2013-10-16 | 石任兵 | Anemarrhenae rhizoma total flavone extract and method for concurrently preparing anemarrhenae rhizoma total flavone extract and anemarrhenae rhizoma total saponin extract |
| CN108239080B (en) * | 2016-12-23 | 2021-09-10 | 中国医学科学院药物研究所 | Mangiferin crystal VI substance, preparation method, composition and application thereof |
| CN108239079B (en) * | 2016-12-23 | 2021-07-06 | 中国医学科学院药物研究所 | Mangiferin crystal V-shaped substance, preparation method, composition and application thereof |
| CN106831909B (en) * | 2016-12-29 | 2019-10-22 | 晨光生物科技集团邯郸有限公司 | The extracting method of double benzene pyrrones compounds in rhizoma anemarrhenae fibrous root |
| CN113416182B (en) * | 2021-05-28 | 2022-03-29 | 西安金泰生物技术有限公司 | Mangiferin and preparation method thereof |
| CN114085883B (en) * | 2021-12-17 | 2023-08-11 | 成都普睿法药物研发有限公司 | Preparation method of timosaponin AIII |
| CN115645340A (en) * | 2022-10-23 | 2023-01-31 | 爱生泽(上海)生物科技有限公司 | Preparation method of rhizoma anemarrhenae total ketone extract and application of rhizoma anemarrhenae total ketone extract in cosmetics |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1844133A (en) * | 2006-04-18 | 2006-10-11 | 广西中医学院 | Process for preparing high purity mangiferin |
| CN101429222A (en) * | 2007-11-05 | 2009-05-13 | 南宁市百济生物工程有限公司 | Method for extracting mangiferin |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1844133A (en) * | 2006-04-18 | 2006-10-11 | 广西中医学院 | Process for preparing high purity mangiferin |
| CN101429222A (en) * | 2007-11-05 | 2009-05-13 | 南宁市百济生物工程有限公司 | Method for extracting mangiferin |
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